CN107382381B - Production process of high-quality potassium magnesium sulfate fertilizer - Google Patents
Production process of high-quality potassium magnesium sulfate fertilizer Download PDFInfo
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- CN107382381B CN107382381B CN201710773333.1A CN201710773333A CN107382381B CN 107382381 B CN107382381 B CN 107382381B CN 201710773333 A CN201710773333 A CN 201710773333A CN 107382381 B CN107382381 B CN 107382381B
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- C05—FERTILISERS; MANUFACTURE THEREOF
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Abstract
A production process of a high-quality potash magnesium sulphate fertilizer comprises the following steps: (1) mixing fresh water and picromerite concentrate obtained by flotation according to a certain proportion, heating and stirring until picromerite concentrate is completely dissolved to obtain liquid l0(ii) a (2) The liquid l obtained in the step (1)0Filtering to obtain filter residue S1And filtrate l1(ii) a (3) Filtering the filtrate l obtained in the step (2)1Carrying out isothermal evaporation crystallization to obtain slurry after crystallization; (4) carrying out constant-temperature solid-liquid separation on the slurry obtained after the crystallization in the step (3) to obtain solid S2And a liquid l2(ii) a (5) The solid S obtained in the step (4)2Drying and dehydrating to obtain the high-quality potassium magnesium sulfate product. The invention has simple process flow and the product K2Compared with the traditional potash magnesium sulphate fertilizer, the content of O is greatly improved, the nutrient proportion is more reasonable, the product granularity is large, the water solubility is good, the quality guarantee period is still longer in an unsealed state, and the additional value is high.
Description
Technical Field
The invention relates to a production process of a potash magnesium sulphate fertilizer, in particular to a production process for processing and extracting a high-quality potash magnesium sulphate fertilizer by utilizing picromerite flotation concentrate.
Background
A potash magnesium sulphate fertilizer with a molecular formula of mK2SO4·MgSO4·nH2O，Wherein m = 1-2, n = 0-6, compared with the traditional potassium sulfate product, the potassium magnesium sulfate fertilizer increases magnesium medium elements, can provide more comprehensive and balanced nutrients for crops, and is more suitable for the growth of economic crops such as vegetables, fruit trees, tobacco, tea leaves, flowers and the like.
At the present stage, the main component of the domestic potash magnesium sulphate fertilizer is soft potassium magnesium vanadium, and the molecular formula is K2Mg(SO4)2·6H2O, the execution standard is GB/T20937-2007, and the superior product requirement is water-soluble potassium (K)2O) is more than or equal to 30 percent, water-soluble magnesium (Mg) is more than or equal to 7 percent, and water-soluble sulfur (S) is more than or equal to 18 percent; first-class requirement is water-soluble potassium (K)2O) is more than or equal to 24 percent, water-soluble magnesium (Mg) is more than or equal to 6 percent, and water-soluble sulfur (S) is more than or equal to 16 percent; the qualified product is water-soluble potassium (K)2O) is more than or equal to 21 percent, water-soluble magnesium (Mg) is more than or equal to 5 percent, and water-soluble sulfur (S) is more than or equal to 14 percent. Due to picromerite K2The content of 0 is low, the potassium, magnesium and sulfur nutrients are not reasonably matched, and the growth effects of various chlorine-avoiding crops are not obvious. Meanwhile, as the potash fertilizer contains more crystal water, the potash fertilizer is easy to deliquesce in the south with humid and sultry climate and cannot be stored for a long time, so that the domestic potash magnesium sulphate fertilizer has lower market acceptance, limited sales and low market price in the potash fertilizer market.
At present, the production method of potassium magnesium sulfate fertilizer in China mainly adopts the processes of conversion, flotation, washing and drying, namely KCl and MgSO in potassium mixed salt raw ore are added with water4·7H2And converting the O into soft potassium magnesium vanadium, enriching the soft potassium magnesium vanadium by adopting a flotation process, and washing and drying the concentrate to obtain a qualified potash magnesium sulphate fertilizer product. When market conditions of potash magnesium sulphate fertilizer products are good, several potash fertilizer production enterprises in Xinjiang and Qinghai produce the traditional potash magnesium sulphate fertilizer products. However, with the continuous low market of potash fertilizers, the price of the traditional potash magnesium sulphate fertilizer is only 1100-1200 yuan/ton, which brings serious loss to production enterprises, the production enthusiasm of the enterprises is not high, the production is stopped at present, and the potassium sulphate is produced by transforming the process.
But the market is different from domestic potash magnesium sulphate fertilizer in that the market is slow to sell and low in price, the imported high-quality potash magnesium sulphate is very pretty, the market price is up to 4600 yuan/ton at present, the potash magnesium sulphate fertilizer is widely welcomed in the potash fertilizer market, and the user evaluation is high. The imported potash magnesium sulphate fertilizer is mainly GermanyThe potassium salt group develops 'red cattle' potassium magnesium sulfate. The difference between the effective nutrient of the fertilizer and the domestic brand potash magnesium sulphate fertilizer is mainly reflected in K2The content of O. The product contains water soluble potassium (K)2O) is more than or equal to 40 percent, water-soluble magnesium (Mg) is more than or equal to 3 percent, and water-soluble sulfur (S) is more than or equal to 18 percent due to K2High content of O and medium element Mg2+、SO4 2-The nutrient matching proportion is reasonable, and the fertilizer is very suitable for the growth of various crops which are forbidden to eat chlorine, such as fruit trees, melons, tobacco, tea leaves and the like, so that the market price of the fertilizer exceeds the price of potassium sulfate. But the imported red bull potassium magnesium sulfate product also has the defects of high content of water-insoluble substances, higher price, inapplicability to drip irrigation fertilization and the like.
In China, potassium sulphate magnesium fertilizer market has various products with different nutrient contents, K2The O content varies from 21%, 24%, 30%, 40%. At present, the domestic market of potash magnesium sulphate fertilizer is lack of 35 percent of K2O, potassium magnesium sulfate fertilizer product. And K2The potash magnesium sulphate fertilizer product with 40 percent of O content is only German 'red bull' potash magnesium sulphate, and at present, K is not available in China2Two novel high-quality potassium sulfate magnesium compound fertilizer production technologies with 35 percent and 40 percent of O content.
In recent years, a plurality of researches on preparing potash magnesium fertilizer products by using potassium mixed salt are reported in literatures, for example, CN101412639A, CN1482102A and the like respectively disclose that the potassium mixed salt is used for producing the traditional potash magnesium sulphate fertilizer by adopting technologies such as two-stage fresh water heating conversion, mechanical screening for removing rock salt, two-stage fresh water normal temperature conversion and the like, but the obtained product has low yield and fine granularity, and the grade only reaches the national standard GB/T20937-2007 qualified product requirement of the potash magnesium sulphate fertilizer; CN101318845A, CN101318844A and the like also disclose a process for extracting potash magnesium fertilizer from potassium mixed salt, wherein the potash magnesium fertilizer is produced by flotation after first-stage fresh water conversion and second-stage fresh water conversion respectively, but the product K2The content of O is not high; the Chinese patent application with the application number of 200710034292.0 utilizes a method of converting potassium mixed salt into fresh water for the first time, carrying out hot melting at high temperature (75-90 ℃) and cooling, and then mechanically screening to remove sodium salt slurry to obtain a coarse-particle (average particle size is more than 3 mm) potassium magnesium fertilizer product, but does not solve the problem of K product2Low O content.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects of the prior art and providing a production process of a high-quality potash magnesium sulphate fertilizer, and the obtained potash magnesium sulphate fertilizer K2High O content, reasonable ratio of potassium, magnesium and sulfur nutrients, large granularity, good water solubility and long shelf life.
The technical scheme adopted by the invention for solving the technical problems is that the production process of the high-quality potassium magnesium sulfate fertilizer comprises the following steps:
(1) mixing fresh water and picromerite concentrate obtained by flotation according to a certain proportion, heating and stirring until picromerite concentrate is completely dissolved to obtain liquid l0；
In the invention, the fresh water is water with the salt content less than or equal to 5 wt%.
(2) The liquid l obtained in the step (1)0Filtering to obtain filter residue S1And filtrate l1；
(3) Filtering the filtrate l obtained in the step (2)1Carrying out isothermal evaporation crystallization to obtain slurry after crystallization;
(4) carrying out constant-temperature solid-liquid separation on the slurry obtained after the crystallization in the step (3) to obtain solid S2And a liquid l2；
(5) The solid S obtained in the step (4)2Drying and dehydrating to obtain the high-quality potassium magnesium sulfate product.
Further, the mass ratio of the picromerite concentrate to fresh water in the step (1) is = 1: 2.5-4.0. Heating until the temperature of the solid picromerite concentrate is completely dissolved is 70-80 ℃. The soft potassium magnesium alum concentrate is a wet material or a dried product, and the ion mass composition of the soft potassium magnesium alum concentrate comprises K+16.42%～24.67%、Mg2+5.37%～7.36%、SO4 2-45.65%～55.49%。
Further, the filter residue S obtained in the step (2)1Water insoluble substances such as silt and the like are discarded as tailings; the filtrate l obtained1The ion mass composition of (A) includes K+4.42%～6.17%、Mg2+1.37%～1.84%、SO4 2-10.63%～13.87%。
Further, the crystallization temperature of the isothermal evaporation crystallization in the step (3) is 70-80 ℃, and the reaction time is 3-5 hours.
Go toAnd (5) performing constant-temperature solid-liquid separation at the temperature of 70-80 ℃ in the step (4). The solid S2Is a wet material, mainly a mixture of potassium sulfate, potassium-magnesium alum and anhydrous potassium-magnesium alum; the ion mass composition of which comprises K+27.73%～32.83%、Mg2+2.70%～5.50%、SO4 2-50.48 to 53.02 percent. The liquid l2The ion mass composition of (A) includes K+1.71%～3.46%、Mg2+6.06%～7.09%、SO4 2-28.18%～30.10%。
Further, the liquid l obtained in the step (5)2Can return to the former part of the potassium mixed salt raw ore to be converted into picromerite section for recycling.
Further, the drying temperature in the step (5) is 280-300 ℃. The effective nutrient content of the obtained high-quality potassium magnesium sulfate product is water-soluble potassium (in terms of K)2O mass) 35-43 percent, and water-soluble magnesium (calculated as Mg)2+Mass) 3.00-6.11 percent, and water-soluble sulfur (based on the mass of S) 17.16-19.94 percent.
The invention has simple process flow and the product K2The content of O is high, the proportion of potassium, magnesium and sulfur nutrients is more reasonable, the product granularity is large, the average grain diameter is 0.2-0.5 mm, the water solubility is good, the mass content of water-insoluble substances is less than 0.1%, the shelf life of a humid and high-temperature climate area (such as 5-8 months in Hunan) in an unsealed state is as long as 1 month, and the added value is high.
Detailed Description
The present invention is further illustrated by the following examples.
In the present specification, the proportions and percentages are by mass unless otherwise specified. In the invention, the fresh water is water with the salt content less than or equal to 5 wt%.
Example 1
The embodiment comprises the following steps:
(1) the chemical mass composition of the picromerite concentrate obtained by flotation in certain potash fertilizer plants is K+16.42%、Mg2+5.37%、SO4 2-45.65%, the other 32.56%; adding the picromerite concentrate into fresh water at a mass ratio of picromerite to fresh water = 1: 2.5, stirring while heating to 70 deg.C to obtain picromerite concentrateDissolving the ore completely to obtain a liquid l0；
(2) Mixing the liquid0Filtering to obtain filter residue S1And filtrate l1. Residue S1Water insoluble substances such as silt and the like are discarded as tailings; filtrate l1Has a chemical mass composition of K+4.69%、Mg2+1.53%、SO4 2-13.04% and the other 80.74%.
(3) The filtrate l1Carrying out isothermal evaporation crystallization operation at 80 ℃ for 3 hours to obtain slurry after crystallization;
(4) filtering the crystallized slurry at a constant temperature of 80 ℃ to obtain solid S2And a liquid l2(ii) a Solid S2(wet basis) has a chemical mass composition of K+32.83%、Mg2+2.70%、SO4 2-52.00%, the other 12.47%; liquid l2Has a chemical mass composition of K+3.46%、Mg2+6.06%、SO4 2-30.10% and others 60.38%.
(5) Mixing the solid S2And (5) drying at the temperature of 300 ℃ to obtain a high-quality potassium magnesium sulfate product. The effective nutrient content is water soluble potassium (expressed as K)2O mass) 43%, water-soluble magnesium (in terms of Mg)2+Mass) 3.00 percent, water-soluble sulfur (by mass S) 19.94 percent, average particle diameter of the product is 0.2mm, and mass content of water-insoluble substances<0.01 percent. The quality guarantee period of the product in a non-sealed state in a high-temperature and humid climate area (such as 5-8 months in Hunan).
Liquid l2Returning to the former stage to convert the potassium mixed salt raw ore into schoenite for recycling.
Example 2
The embodiment comprises the following steps:
(1) the quality composition of soft potassium magnesium alum concentrate ions obtained by flotation in certain potash fertilizer plant is K+22.12%、Mg2+6.87%、SO4 2-53.17%, the other 17.84%; adding the picromerite concentrate into fresh water at a mass ratio of picromerite to fresh water = 1: 4.0, stirring while heating to 75 deg.C to completely dissolve picromerite concentrate to obtain liquid l0。
(2) Mixing the liquid0Filtering to obtain filter residue S1And filtrate l1. Residue S1Water insoluble substances such as silt and the like are discarded as tailings; the filtrate l obtained1Has a chemical mass composition of K+4.42%、Mg2+1.37%、SO4 2-10.63% and the other 83.58%.
(3) The filtrate l1Carrying out isothermal evaporation crystallization operation at 75 ℃ for 4 hours to obtain slurry after crystallization;
(4) filtering the crystallized slurry at a constant temperature of 75 ℃ to obtain solid S2And a liquid l2(ii) a Solid S2(wet basis) has a chemical mass composition of K+30.93%、Mg2+4.01%、SO4 2-53.02%, others 12.04%, liquid l2Has an ion mass composition of K+2.19%、Mg2+6.87%、SO4 2-29.55% and the other 61.39%.
(5) Mixing the solid S2Drying at 280 deg.C to obtain high-quality potassium magnesium sulfate product with effective nutrient content of water-soluble potassium (K)2O mass) 40.50%, water-soluble magnesium (in terms of Mg)2+Mass) 4.46 percent, water-soluble sulfur (by mass S) 19.64 percent, average particle diameter of the product is 0.3mm, and anhydrous insoluble matter content<0.1 percent. The quality guarantee period of the product in a non-sealed state in a high-temperature and humid climate area (such as 5-8 months in Hunan).
(6) Liquid l2Returning to the former stage to convert the potassium mixed salt raw ore into schoenite for recycling.
Example 3
The embodiment comprises the following steps:
(1) the chemical mass composition of the picromerite concentrate obtained by flotation in certain potash fertilizer plants is K+24.67%、Mg2+7.36%、SO4 2-55.49%, the other 12.48%; adding the picromerite concentrate into fresh water at a mass ratio of picromerite to fresh water = 1: 4.0, stirring while heating to 80 deg.C to completely dissolve picromerite concentrate to obtain liquid l0；
(2) The liquid l obtained in the step (1)0Filtering to obtain filter residue S1And filtrate l1. Filtering residueS1Water insoluble substances such as silt and the like are discarded as tailings; filtrate l1Has a chemical mass composition of K+6.17%、Mg2+1.84%、SO4 2-13.87% and the other 78.12%.
(3) The filtrate l1Carrying out isothermal evaporation crystallization operation at 80 ℃ for 5 hours to obtain slurry after crystallization;
(4) filtering the crystallized slurry at a constant temperature of 80 ℃ to obtain solid S2And a liquid l2(ii) a Solid S2(wet basis) has a chemical mass composition of K+27.73%、Mg2+5.50%、SO4 2-50.48%, others 16.29%, liquid l2Has a mass composition of K+1.71%、Mg2+7.09%、SO4 2-28.18% and the other 63.02%.
(5) Mixing the solid S2Drying at 280 deg.C to obtain high-quality potassium magnesium sulfate product with effective nutrient content of water-soluble potassium (K)2O mass) 35.00%, water-soluble magnesium (in terms of Mg)2+Mass) 6.11 percent, water-soluble sulfur (by mass S) 17.16 percent, average particle diameter of the product is 0.5mm, and anhydrous insoluble matter content<0.05 percent. The quality guarantee period of the product in a non-sealed state in a high-temperature and humid climate area (such as 5-8 months in Hunan).
Liquid l2Returning to the former stage to convert the potassium mixed salt raw ore into schoenite for recycling.
Claims (7)
1. A production process of a high-quality potash magnesium sulphate fertilizer is characterized by comprising the following steps:
(1) mixing fresh water and picromerite concentrate obtained by flotation according to a certain proportion, heating and stirring until picromerite concentrate is completely dissolved to obtain liquid l0(ii) a Heating to the temperature of 70-80 ℃ for completely dissolving the solid picromerite concentrate; the soft potassium magnesium alum concentrate is a wet material or a dried product, and the ion mass composition of the soft potassium magnesium alum concentrate comprises K+16.42%～24.67%、Mg2+5.37%～7.36%、SO4 2-45.65%～55.49%；
The fresh water is water with the salt content of less than or equal to 5 wt%;
(2) the liquid l obtained in the step (1)0Filtering to obtain filter residue S1And filtrate l1；
(3) Filtering the filtrate l obtained in the step (2)1Carrying out isothermal evaporation crystallization to obtain slurry after crystallization; the crystallization temperature of the isothermal evaporation crystallization is 70-80 ℃, and the reaction time is 3-5 hours;
(4) carrying out constant-temperature solid-liquid separation on the slurry obtained after the crystallization in the step (3) to obtain solid S2And a liquid l2；
(5) The solid S obtained in the step (4)2Drying and dehydrating to obtain the high-quality potassium magnesium sulfate product.
2. The production process of the high-quality potash magnesium sulphate fertilizer according to claim 1, wherein the weight ratio of picromerite concentrate to fresh water in the step (1) is = 1: 2.5-4.0.
3. The production process of the high-quality potash magnesium sulphate fertilizer of claim 1 or 2, wherein the filter residue S obtained in step (2)1Is water insoluble and is discarded as tailings; the filtrate l obtained1The ion mass composition of (A) includes K+4.42%～6.17%、Mg2+1.37%～1.84%、SO4 2-10.63%～13.87%。
4. The production process of the high-quality potash magnesium sulphate fertilizer of claim 1 or 2, wherein the temperature of the constant temperature solid-liquid separation in the step (4) is 70-80 ℃.
5. The process for producing high-quality potash magnesium sulphate fertilizer of claim 1 or 2, wherein the solid S of step (4)2Is a wet material, mainly a mixture of potassium sulfate, potassium-magnesium alum and anhydrous potassium-magnesium alum; the ion mass composition of which comprises K+27.73%～32.83%、Mg2+2.70%～5.50%、SO4 2-50.48%～53.02%。
6. Production of high quality potash magnesium sulphate fertilizer according to claim 1 or 2Process, characterized in that the liquid l of step (4)2The ion mass composition of (A) includes K+1.71%～3.46%、Mg2+6.06%～7.09%、SO4 2-28.18%～30.10%。
7. The production process of the high-quality potash magnesium sulphate fertilizer of claim 1 or 2, wherein the drying temperature in the step (5) is 280-300 ℃.
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| CN108516872A (en) * | 2018-06-07 | 2018-09-11 | 国投新疆罗布泊钾盐有限责任公司 | A method of improving powder potash magnesium sulphate fertilizer granularity |
| CN110128175A (en) * | 2019-06-25 | 2019-08-16 | 中国科学院青海盐湖研究所 | A method of potash magnesium sulphate fertilizer raw material is prepared using mine containing potassium and tail salt water |
| CN110128176A (en) * | 2019-06-25 | 2019-08-16 | 中国科学院青海盐湖研究所 | A method of potash magnesium sulphate fertilizer is prepared using mine containing potassium |
| CN110590466B (en) * | 2019-10-31 | 2022-05-20 | 中蓝长化工程科技有限公司 | Production process of full-water-soluble potassium-magnesium slow release fertilizer |
| CN112479748A (en) * | 2020-12-31 | 2021-03-12 | 国投新疆罗布泊钾盐有限责任公司 | Preparation process of full-water-soluble high-potassium potash magnesium sulphate fertilizer |
| CN114292144A (en) * | 2022-02-21 | 2022-04-08 | 吴迪 | Potassium magnesium sulfate fertilizer and preparation method thereof |
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